KR100751948B1 - Method for production of fat removal-edible powder and fat removal-edible powder thereof - Google Patents

Abstract

The present invention relates to degreasing powder prepared by efficiently removing lipids without denaturing the main components of edible oil and fat, and using a hexane as a solvent to extract edible fat and oil from a continuous countercurrent method. Or by using a supercritical fluid, there is an excellent effect of providing degreasing powder that is free of lipids, does not cause denaturation of other components, and is completely free of pesticides.

Degreasing, degreasing powder, sesame powder, supercritical, hexane, edible oil, high protein, high fiber, high calcium

Description

Method for producing edible degreasing powder and degreasing powder produced therefrom {Method for production of fat removal-edible powder and fat removal-edible powder

1A shows a continuous countercurrent lipid removal process using hexanes.

① Continuous countercurrent extractor with rotating multiple blades

② Dryer ③ Raw powder in

④ solvent out ⑤ solvent in

⑥ Degreasing powder ⑦ Dried degreasing powder

⑧ Screw Conveyor ⑨ Line Pump

⑩ 0.1mm filtration SUS screen

1B is an enlarged view of a portion of a 0.1 mm filtered SUS screen.

1C is a partially enlarged view of the screw conveyor (8).

2 illustrates a lipid removal process using a supercritical fluid.

① Extractor ② Pressure reducer

③ Supercritical Fluid-Oil Separator ④ Cooler

⑤ Liquid tank for liquefied fluid (CO ₂ etc.) ⑥ Supply tank for fluid (CO ₂ etc.)

⑦ Supercritical fluid (CO ₂ etc.) circulation pump ⑧ Heat exchanger

⑨ Geological removed

3 is a graph showing the change in lipid removal efficiency (%) when the extraction temperature is changed to 35 to 100 ° C. after fixing the extractor's pressure to 350 bar pressure when removing lipid with supercritical carbon dioxide.

Figure 4 is a graph showing the change in lipid removal efficiency (%) when the pressure is changed to 100 ~ 500 bar after fixing the extraction temperature of the extractor at 70 ℃ when removing lipid with supercritical carbon dioxide.

The present invention relates to a method for producing low fat high protein skim powder, and more particularly, to a method for producing skim powder containing a high content of protein and fiber by removing fat components from edible fat and oil raw materials.

According to the definition of the Food Code, edible oils and fats are soybean oil, corn oil, rapeseed oil, rice bran oil, sesame oil, perilla oil, safflower oil and sunflower, which are manufactured and processed from raw oils obtained from plants (including crushed powder) or animals containing fats and oils. It refers to oil, cottonseed oil, peanut oil, olive oil, palm oil, palm oil, mixed cooking oil, refined common oil, shortening, margarine, red pepper seed oil, and other edible oils (excluding cod liver oil). Edible oils and fats are generally a general term for edible oil (liquid at room temperature) and fat (solid at room temperature). Vegetable edible oil is generally called edible oil. Edible oils and fats are applied to bread (butter, margarine) and dressing (vegetable oil) in addition to cooking such as tempura (vegetable oil, lard, shortening), stir-fry (various oils).

Edible oils and fats are classified into vegetable oils and animal oils according to raw materials. Processed fats and oils made from new fats and oils are called processed fats (margarine, shortening, powder fat, etc.). Vegetable oil is divided into fried oil and salad oil according to the degree of refinement, and may be divided into two kinds of refined oil and salad oil, depending on the type such as safflower and corn. Refined oil is usually refined edible oil one more time, salad oil does not harden to oil state for a certain period of time in cold test, and there are prescribed standards such as acid value and color tone in each type and stage.

Vegetable oils are classified according to the drying rate, which is one of chemical characteristics, from fast drying to dry oils (those having an iodine value of 130 or higher; linseed oil, safflower oil, safflower oil, etc.), semi-dry oils (from iodine value of 130 to 100; cottonseed oil, rapeseed oil, soybean oil, rice bran oil, sesame oil, etc., and undried oil (with iodine value of 100 or less; peanut oil, olive oil, camellia oil, etc.). Among vegetable fats and oils, solids at room temperature are classified as solid fats (palm oil, palm oil, cacao fat, etc.). The vegetable oil has a taste that has its own characteristics depending on the raw materials. Sesame oil is squeezed from sesame seeds. It has a strong aroma and tastes good. It contains a lot of antioxidants called sesamoline and vitamin E (tocopherol). When cooking, no tablets are added to add aroma, leaving a distinctive taste and color tone. Soybean oil is derived from soybeans, also known as soybean oil. It is a raw material of salad oil, fried oil and margarine. There are many other varieties, including peanut oil, corn oil, corn oil, rice bran oil, sunflower oil, and safflower oil. Fried oil is made by mixing two or three vegetable edible oils to taste good when fried. Animal edible oils include refined lard, butter and liver oil. In addition, fish oil, light oil (whale oil), and general vegetable fats and oils are hydrogenated hydrogenated oils, and are used as raw materials for processed fats such as shortening and margarine.

The main component of edible oils and fats is fat. Many fats consist of glycerin and fatty acids and are characterized by these fatty acids. In general, vegetable fats and oils contain many unsaturated fatty acids (including double-bonded carbon), and animal fats and oils contain many saturated fatty acids. But fish oil is high in unsaturated fatty acids. Fats and oils vary depending on the nature and amount of these fatty acids.

Edible oils and fats are used as energy sources in the body. It has about twice as much energy as protein or carbohydrates. As nutrients, essential fatty acids (linoleic acid, linolenic acid, arachidonic acid, etc.) and vitamin E are supplied and mainly contained in vegetable oils and fats. Animal fats, on the other hand, contain cholesterol and saturated fatty acids, and excessive intake causes arteriosclerosis and hypercholesterolemia. Although fat is nutritionally important, increasing fat intake, especially animal fat intake, is a problem these days. It is important to take the right amount in balance without biasing the animal. Linoleic acid is attracting attention in order to prevent and improve arteriosclerosis and hypercholesterolemia, a major cause of adult disease. For this reason, sesame oil, rice bran oil, safflower oil, etc., are particularly treated as health foods high in linoleic acid. Recently, eicosapentaenoic acid (EPA), an unsaturated fatty acid contained in fish oil, is known to prevent blood clots and improve hyperlipidemia. Linoleic acid and other health-friendly fats, but also oxidized, excessive intake causes problems.

Sesame is a perennial herbaceous plant ( Sesamun indicum ) belonging to Sesamum in the Pedaliaceae . Seeds are used as food. Sesame is recognized as a particularly valuable flow food among flow plants, which is not known for some time, but is known as a healthful food with various medicines. In the 3rd century BC, China's intentional book, "Nongxon Chachoeng," sesame seeds are a food that restores the function of the kidneys to revitalize the body, strengthens the function of the five intestines, energizes, strengthens the body, promotes growth, It is written to make good.

The main ingredients of sesame seeds are slightly different depending on the region and harvest time, but they are composed of 52% lipid, 24% protein, 15% sugar, and 3% fiber. According to the amino acid composition of sesame protein, the essential amino acid of sesame seeds satisfies the FAO requirements, and in particular, methionine, arginine, and tryptophan have many characteristics. In addition to these, calcium is present in about 1%, much more than 0.02% of flour, 0.01% of rice or 0.2% of soybeans. Other trace ingredients are rich in iron, selenium, vitamins, etc. B1, B2, etc. are quite abundant and E is also abundant.

Perilla is a perennial plant of the moss family of nectar and is native to Southeast Asia, about 1m tall, with long hairs, squares, straight branches, and has a peculiar smell. The leaves are opposite each other, broad oval-shaped, pointed at the end, rounded at the bottom, and have dull teeth at the edges. The flowers are inflorescences and many white and small lip shaped flowers bloom. Fruits are four small branches perched under calyx, almost ball-shaped, with smooth net surface. It is divided into several species according to the morphological characteristics of the fruit. In Korea, almost brown berries are grown. Seeds are roasted with sesame salt or with oil. Other uses include paints, varnishes, linoleum, printing inks, pomades and soaps. It is widely distributed in Korea, China, India, and Japan.

Perilla helps heal viral bronchitis, stomach ulcers, and colds. In addition, it contains a lot of vitamin E, which helps to improve fertility, vision recovery, prostate treatment, hair loss control, gout prevention, gallstone dissolution. Perilla has a coughing effect and is known to quench thirst and strengthen the cranial nerves. In addition, there is a function to clear the hair was used by the ancient scholars.

Currently, sesame or perilla is mainly used for producing sesame oil or perilla oil, and sesame gourd or perilla seed is produced as a by-product, and is mainly used for animal feed. The reason why sesame or perilla is not used for food is that most of sesame oil or perilla oil are squeezed by compression method, so the skim is brown and protein is denatured. Therefore, most of them are used as feed, and the food is hardly progressed.

As described above, the sesame or perilla sesame foil contains a lot of protein, sugar and fiber, and moreover, there are many sulfur-containing amino acids that are easily lacking in plant foods.

In addition, the saccharides of sesame seeds contain about 0.2% of lignans as glycosides, which are decomposed by enzymes in vivo to become free lignan compounds (sesaminol or pinorenol), which show strong antioxidant activity (H. Katsuzaki, et al., Biosci. Biotech.Biochem. , 56, 2087 (1992)).

Therefore, food resourceization of skim cakes is worthwhile and urgent. Soybeans and corn are also highly used for protein and starch along with oil, but degreasing foil produced as a by-product of edible fats and fats by current hot pressing method is not suitable for edible use. This is because of the severe browning and protein denaturation by the method, and since it still contains about 20% fat even after pressing, it is not suitable for the taste of modern people who prefer low-fat foods.

Accordingly, the present inventors have made diligent efforts to effectively remove only fat components without denaturing other nutrients of edible fats and oils, and to prepare skim degreasing powder rich in proteins, dietary fiber, calcium and vitamins, resulting in a diameter of 1.25. The edible oil and fat powder crushed in mm was carried out by a continuous countercurrent method using hexane as a solvent, or by using a supercritical fluid to find that lipids were removed with high efficiency, thereby completing the present invention.

In order to achieve the above object, the present invention provides a method for producing skim powder, characterized in that using the edible oil powder prepared by crushing the edible oil and fat raw material in the method for removing the lipid from the edible fat and oil raw material. do.

As a raw material to which the method for preparing skim powder of the present invention can be applied, any raw material capable of manufacturing skim powder known in the art may be used. Specific examples of skim powder that can be produced by applying the method of the present invention include sesame skim powder, perilla skim powder, soybean skim powder, safflower skim powder, corn skim powder, rice skim powder, peanut skim powder, sunflower seed skim powder, etc. have.

The edible oil and fat raw material may be subjected to a pretreatment step before removing the lipids, treatment to remove harmful substances such as microorganisms, residual pesticides and preservatives on the surface of the raw material, treatment to increase the contact area with the supercritical fluid, extraction Treatments to increase efficiency and treatments to increase the sensuality of the edible oils and fats.

As the treatment for removing harmful substances, methods such as ultraviolet irradiation and heat treatment can be used, and as a treatment for increasing the contact area, a grinding method can be used. In order to increase the extraction efficiency, sesame seeds and perilla can be heat-treated to remove 5 ~ 10% of moisture to increase the extraction efficiency of oils and fats. In this case, the extraction efficiency can be increased by going through a drying process. As a treatment for increasing the sensory beauty of degreasing powder, a method such as far-infrared irradiation can be used.

In the present invention, UV irradiation may be performed for 1 hour or more, but preferably performed for 1 to 3 hours, and heat treatment may be performed at 80 ° C. or more for 30 minutes or more in terms of removing harmful substances or functionalities, and preferably at 180 to 220 ° C. It is preferable to perform 15 to 40 minutes, more preferably 15 minutes at 220 ℃. Soybean, olive, peanut, safflower seed drying process is preferably carried out at 100-120 ℃ until the water content reaches 0.1-0.2%, most preferably at 110 ℃ until the water content reaches 0.18% It is good. Moisture content can be measured with a commercially available moisture meter.

The edible oil and fat raw material powder used in the present invention is preferably a particle size of 0.42 ~ 1.25mm.

In the present invention, in order to overcome the disadvantage that the inherent scent of the raw material is increased by the loss in the process of heat treatment at a high temperature can be irradiated with far infrared rays during the heat treatment.

In the present invention, the far-infrared irradiation can be used any method known in the art, the emissivity (5 ~ 20㎛) is 0.8 ~ 0.9, the radiation energy (W / ㎡) is preferably about 3.5 × 10 ² ~ 3.8 × 10 ² Most preferably, the emissivity (5-20 μm) is 0.913, and the radiation energy (W / m 2) is about 3.68 × 10 ² .

When edible oil was crushed to less than 0.42mm before lipid removal, the amount of crushed powder decreased when extracting nucleic acid, but the mass transfer rate increased, but the descending rate of the sample decreased compared to the lift force of the multi-stage blade. The degreasing edible oil and fat powder is also removed during the exchange, so that the yield is not only reduced, but the sedimentation rate of the powder is too slow to be suitable for continuous operation. In addition, during supercritical extraction, there is a problem of stopping operation due to pressure drop by blocking the upper membrane, and clogging of the valve and line of the supercritical device by the micro powder passing through the upper membrane. .

If the average diameter is 1.25 mm or less, the lipid removal efficiency is preferably higher than 99% for nucleic acid extraction and supercritical fluid extraction.

On the other hand, preferably in the method for producing skim powder, the removal of lipids is removed by a continuous countercurrent extraction device using hexane as a solvent or by supercritical extraction using a supercritical fluid such as supercritical carbon dioxide as a solvent. It is good.

On the other hand, more preferably, the continuous countercurrent extraction device is provided with a screw conveyor (8) at the lower end of the raw material discharge portion gradually decreasing in diameter toward the end, and has a line pump (9) on one side, raw material discharge The inner peripheral surface of the negative portion is preferably provided with a 0.1mm filtration SUS screen (10) essentially. The screw conveyor (8), the line pump (9), the 0.1mm filtration SUS screen 10 is provided to remove the solvent mixed in the degreasing powder is made at the same time with the extraction is possible a continuous process.

As the supercritical fluid in the present invention, carbon dioxide, nitrogen, nitrous oxide, methane, ethylene, propane and propylene may be used. Among them, it is preferable to use supercritical carbon dioxide, wherein the input temperature is 31 to 200 ° C, and the input pressure is 100 to 900 bar.

On the other hand, the method of using the supercritical fluid of the present invention is one of the technologies using the advantages of the supercritical fluid, since the principle of distillation and extraction is a complex technology that is applied at the same time It has several unique advantages. That is, since the supercritical fluid can be set to any condition of high density to low density by manipulation of the pressure and temperature, it is excellent in selectivity such as fractionation and separation, so that a high purity product can be obtained, and the extraction solvent is almost completely lost. It can be easily recovered, and there is an advantage in that a purified product having no residual solvent can be obtained. In addition, the viscosity of the supercritical fluid is small, so it penetrates into the sample, and the extraction efficiency is high. Also, the diffusion coefficient is large, so the extraction speed is high. Since the density difference between the sample and the supercritical fluid is large and the viscosity of the supercritical fluid is low, the extraction residue and the solvent can be easily separated. However, the edible oil and oil removal means using the supercritical fluid has a disadvantage that it requires a high pressure device, so the cost of facility and maintenance is high, and the extraction using the supercritical fluid has been confirmed to be economical only with high efficiency.

Carbon dioxide in supercritical fluids is most preferred because its critical pressure is 73.8 bar and its critical temperature is 31 ° C., which is why it is generally easy to create supercritical conditions, because it is nontoxic and inexpensive to carbon dioxide itself. In addition, supercritical carbon dioxide is a nonpolar solvent and is preferable for extraction of substances having low polarity, such as fats and oils.

On the other hand, in the supercritical extraction, the supercritical carbon dioxide is preferably at a temperature of 31 to 200 ° C. and at a pressure of 100 to 900 atm, and more preferably at a pressure of 300 to 550 at a temperature of 40 to 80 ° C. . From above 31 ℃, carbon dioxide is changed to supercritical state, so supercritical extraction is possible. After above 40 ℃, the extraction efficiency is increased. If it exceeds 80 ℃, the extraction efficiency is not increased but it is still high. Extraction efficiency It is possible to extract at more than 100 atm, and the extraction efficiency is increased above 300 atm. If it exceeds 550 atm, there is no increase in extraction efficiency compared to the previous one, but still has a high extraction efficiency.

On the other hand, preferably, the edible oil and fat raw material is preferably heated at 60 ° C or more immediately before being extracted into the supercritical fluid, preferably at 60 to 200 ° C, more preferably at 80 to 200 ° C. In addition, the edible oil and fat raw material is preferably crushed, preferably crushed to 1.50mm or less, and more preferably crushed to 0.42 ~ 1.25mm size.

If the temperature of the supercritical fluid to be extracted is lower than that of filling the sample, the sample will shrink than the original. As the sample shrinks, the space between the samples in the extractor increases. At this time, the supercritical fluid rising between the samples flows in a wider space when filling, thereby decreasing the flow rate. If the flow rate is lower than the original, the chance of the microparticles rising with the supercritical fluid is reduced, so that the upper filter is not blocked. Therefore, when supercritical carbon dioxide is used as a fluid, when the temperature of the supercritical carbon dioxide is lowered to around 31 ° C., the edible fat or oil may be heated to a low temperature near 60 ° C. immediately before extraction, but should be set higher than the temperature of the supercritical fluid. . Therefore, when using a supercritical fluid of 40-80 ° C. in consideration of extraction efficiency, the sample temperature is not preferable because the shrinkage of the sample is less than 80 ° C., while the edible fat and oil is burned above 200 ° C., which is not preferable. .

In addition, the present invention provides a skim powder from which the lipid is removed by any one of the above extraction method.

Sesame seeds used in the following examples of the present invention contain 51.9% as a main component of lipids. Others contain 24.5% protein, 15.1% sugar and 3.1% fiber.

In the present invention, to remove lipids efficiently, but to prevent denaturation or loss of other components, edible fats and raw materials such as sesame seeds were made easy to extract, and extracted with hexane.

Hexane is a safe solvent used in the production of soybean cooking oil and has excellent lipid extraction efficiency. In addition to hexane, efficient extraction was possible even with the use of supercritical carbon dioxide, which has recently been spotlighted as a clean solvent. In addition, the supercritical carbon dioxide is advantageous because there is a characteristic that no residual solvent remains after extraction.

For the following examples, the superiority of the method and apparatus for preparing skim powder of the present invention was verified through actual experiments, and the results are shown in the following tables.

Hereinafter, the configuration and operation of the present invention will be described in more detail with reference to the following experiments and examples, but the scope of the present invention is not limited only to the following examples.

Example 1 Pretreatment of Edible Fats and Oils for Efficient Removal of Lipids

Sesame, perilla and peanut were used as raw materials to measure lipid extraction removal efficiency while changing the properties of the raw materials. The raw material was extracted in hexane and supercritical carbon dioxide in the form of seed, pressed flakes and crushed fine particles, and the residual lipid content was measured.

Hexane extraction was carried out by filling 200 ml of hexane in the reactor (Fig. 1), and then adding 5 g of the raw material forms described in Tables 1 to 3 per minute, and replacing the hexane with fresh solvent by 20 ml per minute. At this time, the rotation speed of the multi-blade and the screw was adjusted to 200rpm. At this time, the height ratio (L / D) to the width of the reactor was 10, the total volume of the reactor was 300ml. This operation was carried out for 1 hour, and the results were shown in Tables 1 to 3.

Supercritical carbon dioxide was carried out at 450 atmospheres 60 ° C. for 3 hours using the apparatus shown in FIG. 2, and this condition was in a supercritical state.

Lipid removal efficiency measured the weight of the extracted and separated lipids, the total amount of lipids contained in the raw material was calculated as 100% and the weight of the removed lipids in percent.

Lipid Removal Efficiency According to the Shape of Raw Sesame Seeds Raw sesame form Lipid Removal Efficiency with Hexanes (%) Lipid Removal Efficiency Using Supercritical Carbon Dioxide (%) Seed form 2.3 2.1 Flake 31.3 27.8 Fine particle form (average diameter 1.25mm or more) 95.6 94.1 Fine particle form (average diameter less than 1.25mm) 99.0 99.5

Lipid Removal Efficiency According to the Shape of Raw Perilla Raw perilla form Lipid Removal Efficiency with Hexanes (%) Lipid Removal Efficiency Using Supercritical Carbon Dioxide (%) Seed form 2.1 1.9 Flake 30.7 25.4 Fine particle form (average diameter 1.25mm or more) 93.9 90.9 Fine particle form (average diameter less than 1.25mm) 98.2 99.3

Lipid Removal Efficiency According to the Type of Raw Peanut Raw peanut form Lipid Removal Efficiency with Hexanes (%) Lipid Removal Efficiency Using Supercritical Carbon Dioxide (%) Seed form 0.5 0.2 Flake 16.4 13.8 Fine particle form (average diameter 1.25mm or more) 93.1 92.6 Fine particle form (average diameter less than 1.25mm) 98.3 99.3

As shown in Table 1 to Table 3, the lipid removal efficiency is greatly affected by the form of the raw material. In particular, the smaller the particle size, the better the efficiency, which is thought to be due to the increased contact area between the raw material and the solvent, thereby increasing the removal efficiency. In the case of seed or fragment form, the removal efficiency is not considered to be high due to diffusion limitation.

Example 2 Continuous Countercurrent Extraction for Increased Lipid Removal Efficiency

When hexane is removed as a solvent, a continuous countercurrent extraction method as shown in FIG. 1A is designed to increase efficiency. The sample is injected from the upper part ③ and the solvent is injected from the lower part ⑤. The sample with a large specific gravity descends, the solvent rises, contact occurs and lipids are extracted. In the center is a rod equipped with several blades. By rotating it, the rate of descent of the sample and the rate of rise of the solvent were controlled. When properly controlled, the contact time between the sample and the solvent was greatly increased, and eventually, the mass transfer rate was increased to increase the efficiency of the lipid extraction agent.

In the case of the conventional batch type, the powder is extracted with a solvent and then the solvent is removed using a filter, and then the filtrate is transferred to a dryer, whereas the continuous countercurrent extraction device of the present invention transfers the submerged degreasing powder through the screw conveyor ⑧. The degreasing powder and the solvent mixture between the pitch of the screw and the pitch while moving to the dryer at the same time as the dryer are manufactured to remove the solvent through the hole of the screen by the centrifugal force of the screw and the ⑨line pump between the ⑩0.1mm filtration SUS screen. It became. Therefore, the removal of the solvent mixed in the degreasing powder is made at the same time it is possible to produce an effective degreasing powder.

After filling 200ml of hexane in the reactor, 5g / min of crushed raw powder passing 95% or more of metal mesh with diameter of 1.25mm was added per minute, and hexane was replaced with fresh solvent by 20ml / min. At this time, the rotation speed of the multi-blade and the screw was adjusted to 200rpm. At this time, the height ratio (L / D) to the width of the reactor was 10, and the total reactor volume was 300 ml. As a result of operating for 60 minutes, the dried sesame powder removed 99% of lipids in the case of sesame seeds, and the dried sesame powder removed 98% of lipids in the case of raw sesame seeds. The powder had 97% lipid removed.

The above-mentioned method has several advantages over the general batch extraction process, which primarily improves the mass transfer rate and the lipid removal efficiency due to continuous current current. In addition, there is no need for multi-stage extraction, which is required for general batch extraction, which simplifies the process and saves space.

Lipid removal experiment using sesame seeds and the above-mentioned method and device showed 98% lipid removal within 10 minutes.

Example 3 High Efficiency Lipid Removal Method Using Supercritical Fluids

When removing lipids with supercritical carbon dioxide, the extraction method as shown in FIG. 2 was designed to increase efficiency. Raw material powder was filled in the extractor ① and lipids were removed using supercritical CO ₂ supplied through the pump ⑦. The lipid to be extracted and removed was fed to the separator ③ after the pressure was lowered through the pressure regulator ② with supercritical CO ₂ . In the separator, the lipids accumulate down in the liquid state and CO ₂ escapes up in the gaseous state. The gaseous CO ₂ was not discarded, but was liquefied in the cooler ④, stayed in the storage tank ⑤, and fed back to the extractor by the circulation pump ⑦ to remove the lipid.

2.5 kg of the crushed raw material powder which passed 95% or more of the metal mesh with a diameter of 1.25 mm was extracted with 25 kg of supercritical carbon dioxide per hour for 3 hours. In the case of sesame seeds, the extraction pressure was changed to 350 bar after fixing the extraction pressure to 350 ~ 100 ℃, the lipid removal efficiency was changed as shown in Figure 3, after fixing the extraction temperature to 70 ℃, the pressure was changed to 100 ~ 500bar lipid Removal efficiency was as shown in FIG. Perilla and peanut also showed the lipid removal efficiency of the same trend as above. In the above results, the lipid removal temperature of the crushed raw powder using supercritical carbon dioxide was more than 40 ° C, more preferably 60 ° C or more, and 300bar, more preferably 450bar or more. As a result, dried skim powder removed up to 99.8% of sesame seeds, up to 99.6% of perilla, and up to 99.3% of peanuts.

When filling a fine sample in a general supercritical fluid extractor and extracting and removing lipids with supercritical carbon dioxide, the fine particles move to the upper part of the extractor to block the upper filter, which intensifies the pressure drop inside the extractor and stops the operation. Cases occur frequently. However, a feature of the present invention is characterized in that the sample is heated to a high temperature of 80 ~ 200 ℃ after filling, and extracted with a supercritical carbon dioxide of 60 ~ 80 ℃, which is much lower than this temperature. If the temperature of the supercritical fluid to be extracted is lower than that of filling the sample, the sample will shrink than the original. As the sample shrinks, the space between the samples in the extractor increases. At this time, the supercritical fluid rising between the samples flows in a wider space when filling, thereby decreasing the flow rate. If the flow rate is lower than the original, the chance of the microparticles rising with the supercritical fluid is reduced, so that the upper filter is not blocked.

Experimenting with the above designed method did not block the filter at all. However, experiments using the conventional method had a 60% chance of clogging the upper filter when operated several times. In addition, the devised method has an excellent result of improving the overall efficiency by eliminating the channeling phenomenon during extraction, which reduces the time for extracting and removing lipids by about 20%.

Experimental Example 1. Degeneration of Protein

Currently, degreasing powder such as sesame skim powder, sesame skim powder, peanut skim powder, etc., produced as a by-product by sesame oil, perilla oil and peanut oil, are inadequate for edible use. Severe browning and protein denaturation are the main causes, and protein denaturation is unsuitable for food use because it can affect safety as a food.

In order to confirm whether the protein denaturation, sesame powder produced by the present invention and sesame powder obtained by the conventional sesame oil production method, that is, the protein component of sesame gourd was analyzed.

Sesame seeds contain so many different types of proteins that you cannot analyze each of them to see if they are denatured. However, analyzing the total or free amino acids in a sample can determine whether the protein is changing in its entirety. In total amino acid analysis, each sample is placed in a 50 mg test tube and hydrolyzed by adding 15 ml of 6 N HCl solution. At this time, the hydrolysis is continued for 24 hours at 105 ℃. After hydrolysis, the solution was diluted to 50 ml, filtered through a 0.2 micro filter, and 200 µl of the filtrate was dried. The dry matter was dissolved in 200 μl of 0.1 N HCl and used for HPLC analysis.

The free amino acid was extracted by adding 5 g of a sample to a 500 ml Erlenmeyer flask and adding 400 ml of 0.005 M HCl. At this time, extraction conditions were extracted for 30 minutes with stirring at 80 ℃. After cooling, distilled water was added to make 500 ml and filtered through a microfilter. 200 μl of the filtrate was dried and dissolved in 100 μl of pure water, followed by OPA derivatization by the above method and analyzed by HPLC.

HPLC analysis conditions were as shown in Table 4 below. The column used CUROSIL PFP (4.6 (250 mm, 5 micron, phenomenex), the solvent conditions A solvent is MeOH: THF: 0.02M sodium acetate (pH5.9) = 20: 2.5: 77.5, v / v B The solvent was MeOH: THF: 0.02M sodium acetate (pH5.9) = 80: 2.5: 17.5, v / v The detection time, solvent A, solvent B and flow rate were as follows.

HPLC analysis conditions Minutes A solvent B solvent Flow rate 0 100 0 1ml / min 2 100 0 1ml / min 15 73 27 1ml / min 35 0 100 1ml / min 40 100 0 1ml / min

The injection amount was 10 mu l, the fluorescence detector was Exitation lambda = 360, Emission lambda = 450 and the column temperature was 40 ℃.

In Table 5 and Table 6, three types of samples were analyzed and compared. The raw material was roasted sesame seeds at 200 ° C. for 30 minutes. As shown in Table 5, the total amino acid content of the skim sesame powder produced by the present invention did not show a large change compared to the raw material, but the sesame gourd produced as a by-product in the existing sesame oil manufacturing method was reduced by 21.5% based on the total content. In addition, specific amino acids were greatly reduced, with aspartic acid, arginine, arginine, serine, and threonine. In particular, arginine decreased by 59%. Table 3 shows the results of free amino acid analysis. In the case of the skim sesame powder produced according to the present invention, only a slight amount of free amino acid content was reduced compared to the raw material. However, the free amino acid content of sesame gourd by the conventional method was greatly reduced, which was reduced by 56.5% based on the total amount. More seriously, other amino acids except proline and valine were not detected. Through these experimental results, the sesame gourd protein remaining after sesame oil production by the conventional method is considered to be severely denatured. In conventional crimping or expeller methods, the temperature of raw sesame seeds is very high during milking, which is thought to be the cause of protein denaturation.

Total amino acids content per sample (mg%, dry base)          Sample amino acids Raw material Sesame gourd Sesame powder (invention) Asp 3785.9 2796.7 3730.5 Glu 9215.6 8233.4 9156.9 Ser 1477.2 302.4 1401.5 His 1077.5 801.8 1072.6 Gly 2541.8 2152.3 2550.1 Thr 1452.9 548.9 1404.6 Ala 2573.1 2455.9 2521.7 Arg 4278.2 1743.6 4220.9 Tyr 1897.4 1871.5 1876.5 Cys 159.5 - 145.7 Val 2317.6 2176.3 2320.9 Met 1354.7 1130.4 1311.3 Phe 2249.1 2010.5 2208.3 IIeu 1802.4 1689.6 1796.4 Leu 3597.5 3582.9 3588.7 Lys 428.6 298.9 413.5 Pro 1854.8 1219.8 1816.6 Total 42,063.8 33,014.9 41,536.7

Free amino acids content per sample (mg%, dry base)          Sample amino acids Raw material (Sesame seeds, 200 ℃ roasting) Sesame gourd (by-product of conventional sesame oil production) Sesame powder (invention) Asp 7.4 - 7.1 Glu - - - Ser - - - His 2.5 - 2.4 Gly 0.5 - 0.6 Thr 1.2 - 0.9 Ala 1.4 - 1.4 Arg 4.2 - 3.9 Tyr - - - Cys - - - Val 4.3 1.9 4.1 Met 3.8 - 3.5 Phe 3.9 - 3.4 IIeu 2.2 - 1.8 Leu 2.3 - 2.1 Lys - - - Pro 40.1 30.2 39.8 Total 73.8 32.1 71.0

Experimental Example 2: Analysis of residual pesticides in skim flour (simultaneous multicomponent analysis)

The presence of pesticide residues in sesame powder among several skim flours was investigated using the following simultaneous multi-component analysis.

(1) 25g of sesame powder from which lipid was removed was taken.

(2) 100 ml of acetonitrile, an extraction solvent, was extracted using a homogenizer.

(3) The acetonitrile solution was filtered using a Buchner funnel and placed in an empty vacuum flask.

(4) 50 ml of acetonitrile, an extraction solvent, was reextracted using a homogenizer.

(5) After filtration using a Buchner funnel, the filtrate was combined with the filtrate collected in step 3 and then proceeded.

(6) The filtrate was concentrated using a vacuum evaporator.

(7) 5 ml of acetone was added to the concentrated sample to dissolve the sample.

(8) 148 residues of pesticides were analyzed using gas chromatography (GC).

Groups I and II were analyzed using gas chromatography / mass spectrometry (GC / MSD) after gas chromatography analysis under the conditions shown in Table 7 below.

Gas chromatography analysis conditions (Table 7) and pesticide names (148 species) used in Screen (Table 8) were as follows.

Analytical conditions for GC (model: hp 6890) division Group (Ⅰ) Group (Ⅱ) Confirm Detector NPD (Model: hp5890) ECD (Model: hp6890) MSD (Model: hp5973) Inlet temp. 260 ℃ 260 ℃ 260 ℃ Detector temperature (Detector Temp.) 280 ℃ 280 ℃ 280 ℃ Flow rate lml / min 1ml / min 1ml / min Column DB-17 (30m × 0.25mm × 0.25㎛) Ultra-2 (50m × 0.2mm × 0.25㎛) HP-5MS (30m × 0.25mm × 0.25㎛) Oven temp. Program 80 ° C (2min) → 10 ° C / min → 280 ° C (15min) 80 ° C (2min) → 10 ° C / min → 280 ° C (25min) 80 ° C (2min) → 10 ° C / min → 280 ° C (10min)

Name of pesticide used in screening (148 species) (1) Group (Ⅰ) No NPD Mix. One NPD Mix. 2 NPD Mix. 3 NPD Mix. 4 NPD Mix. 5 One Ethion Edifenphos Dimethylvinphos Chlorfenapyr Pyraclofos 2 Thiometon Pirimicarb Omethoate Diphenylamine Pyridaben 3 Isofenphos Prometryn Diethofencarb Fenobucarbo Tebufenpyrad 4 Mecarbam Triadimefon Cresoxim-methyl Fipronil Isoprothiolane 5 Parathion Thiobencarb Metaaxyl Fludioxonil 6 Pirimphos-ethyl Flusilazole Alachlor Iprobenfos 7 Carbophenothion Cyprodinil Oxadiazon Tebutryn 8 Pirimphos-methyl Chlorfenvinphos Simazine Prothiofos 9 Tolclofos-methyl Tolyfluanid Fenoxycarb Fenothiocard 10 Parathion-methyl Diphenamid Paclobutrazol Cadusafos 11 Triaphophos Fosthiazate Bendicarb 12 Pyrazophos Fenamiphos Carbofuran 13 Penazaquin Vamidothion Mepanipyrim 14 Tricyclazole Espprocarb 15 Tebufos Etoxazole 16 Cyproconazole 17 Mepronil

(2) Group (Ⅱ)

No. ECD Mix. One ECD Mix. 2 ECD Mix. 3 ECD Mix. 4 ECD Mix. 5 One Ethalfluralin Nitrapyrin Mevinphos Diuron Chlordane 2 α-BHC γ-BHC Diazinon Ethoprophos Triflumizole 3 Dicloran Chrorothalonil Metobrorouson Dimethoate Trifuralin 4 Quintozene Vinclozolin Propanil β-BHC o.p＇-DDD 5 δ-BHC Fenitrothion Acetochlor Disulfoton o.p＇-DDE 6 Mettribuzin Diclofluanid Marathion Etrimfos Hexaconazole 7 Chlorpyrifos-Me Chlorpyrifos Metolachlor Penthion Nuarimol 8 Heptachlor Penconazole Dicopol Captan Nonachlor (trans) 9 Broromacil Phenthoate Pendimethalin Oxadixyl Nonachlor (cis) 10 Aldrin Folpet Methidathion Dinocap 11 Heptachlor-epoxide Prolenofos Butachlor Carboxin 12 Procymidone Oxyfluorfen Chrorobenzilate Azinphos-Me 13 Tralomethrin o.p＇-DDT Phosmet Permethrin 14 α-Endosulfan Endosulfan-sulfate Posalone Fenbuconazole 15 p.p＇-DDE Diclofop-Me Cyfluthrin Microbutanil 16 Dieldrin Captapol Cypermethrin 17 Endrin Bifenthrin Fenvalerate 18 β-Endosulfan Bromopropylate Fluvalinate 19 p.p＇-DDD Methoxychlor Deltamethrin 20 p.p＇-DDT Penarimol

21 Iprodione Prochloraz 22 EPN Sinomemethionat 23 Tetraradifon 24 λ-cyharothrin

As a result, no pesticides were detected.

Experimental Example 3: Sensory evaluation of degreasing powder prepared by the method of the present invention

Sesame, perilla and peanut among edible oils and raw materials were washed with water, and then sesame and perilla were roasted at 220 ° C. for 15 minutes and dried at 110 ° C. until the water content reached 0.18%. Irradiated dried peanuts were irradiated with ultraviolet rays for 1 hour to remove contaminants such as microorganisms, and then irradiated with far infrared rays having an emissivity (5 ~ 20㎛) of 0.913 and radiation energy (W / ㎡) of 3.68 × 10 ² for 1 hour The sesame skim powder, perilla skim powder and peanut skim powder were prepared by extracting and removing lipids for 3 hours using 60 ° C. and 450 atm of supercritical carbon dioxide. Sesame skim powder, perilla skim powder and peanut skim powder prepared by the present invention prepared as described above and sesame skim powder, perilla skim powder and peanut skim powder produced by conventional crimping, as a control, 20 consumers as a sample The evaluation result of preference was as follows Tables 9-11. Through the following Tables 9 to 11 it was confirmed that the degreasing powder according to the method of the present invention is much superior to the crimping in the functional aspect.

Sesame skim powder test results Comprehensive sensory incense Savory taste bitter color Invention 17 people 19 people 15 people 5 people 20 people Control 3 people 1 person 5 people 15 people 0 people

Perilla degreasing powder test results Comprehensive sensory incense Savory taste bitter color Invention 19 people 19 people 20 people 3 people 20 people Control 1 person 1 person 0 people 17 people 0 people

Peanut Skim Powder Test Results Comprehensive sensory incense Savory taste bitter color Invention 19 people 20 people 19 people 4 people 20 people Control 1 person 0 people 1 person 16 people 0 people

As described above, the present invention can provide a method for preparing skim powder in which lipids are removed from edible fat and oil raw materials with high efficiency, but do not cause degeneration of other components, and pesticides are completely removed. The skim powder obtained through the present invention is a high protein food having a high protein content. In addition, since the protein contained in the lipid removal process of the present invention is not denatured, the skim powder of the present invention has the advantage of being used as an excellent food. Moreover, the high content of fiber and calcium can provide a high fiber and high calcium food. It is a very useful invention in the food industry because it has an excellent effect.

Claims (2)

Drying any one of the edible fats and oils selected from the group consisting of safflower seeds, corn, rice, peanuts and sunflower seeds at 100-120 ° C. until the water content reaches 0.1-0.2%; Irradiating ultraviolet rays to the edible fat and oil raw material dried in the step; Irradiating far infrared rays to the edible oil and fat raw material irradiated with ultraviolet rays in the step; Crushing the far-infrared irradiated edible oil and fat raw material to a size of 0.42 to 1.25 mm; And Lipids are removed from the edible fats and fats crushed in the above step by using a supercritical extraction method using a supercritical fluid selected from the group consisting of carbon dioxide, nitrogen, nitrous oxide, methane, ethylene, propane and propylene as a solvent. Degreasing powder produced by the manufacturing method comprising the step of improving the functional beauty. delete

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